Alloy and process of producing the same.



UNITED STATES PATENT OFFICE.

JOHN LOUIS BROWN, OF BALTIMORE, MARYLAND, ASSIGNOR TO EDWARD R. COOPER,OF BALTIMORE, MARYLAND.

ALLOY AND PROCESS OF PRODUCING THE SAME.

No Drawing.

b all whom it may concern:

Be it known that I, JOHN LOUIS BROWN, a" citizen of the United States,residing at Baltimore, in the State of Maryland, have invented certainnew and useful Improvements in Alloys and Processes of Producing theSame, of which the following is a specification.

This invention relates to alloys and processes of producing the same;and it comprises as a new article an alloy comprising zirconium andiron, said alloy containing advantageously between 40 and 90 per cent.of zirconium with the residue mainly iron, or an iron group metal, andsaid alloy also advantageously comprising a certain amount of titanium,and also comprising in certain cases a small amount of aluminum or othermetal; and it also comprises a filament or other luminescent bodycomposed of said alloy and it further comprises a method of producingsuch alloys wherein zirconium and iron compounds are co-reduced in thepresence of sufficient titanium compounds to produce certainadvantageous effects and to insure the entry of a small amount ofmetallic titanium into the alloy produced; all as more fully hereinafterset forth and as claimed. 7

Numerous attempts have been made to obtain alloys of zirconium whichcould be worked up into forms commercially useful, but such attemptshave been heretofore largely unsuccessful. Zirconium itself is a hard,brittle substance existing in several allotropic forms, all of which areeasily fractured and possess little or no ductility or malleability.These properties have also characterized practically all the alloys ormetal mixtures heretofore produced in which zirconium was present inmore than comparatively small proportions. Moreover it has been foundextremely difficult to alloy zirconium with other metals by directaddition of the one metal to the other with production of uniform andhomogeneous ductile and malleable alloyed products; products which aresusceptible of being treated by metal-working processes such as drawing,forging, rolling, casting, and the like. The physical and chemicalproperties of these directly produced alloys prevent such manipulation.

According to the present invention true Specification of Letters Patent.

Patented Aug. 24, 1915.

Application filed January 22, 1912. Serial No. 672,707.

alloys of zirconium with iron, or another metal of the iron family, areproduced by the simultaneous reduction of the constituent metals fromcompounds containing them. Under these conditions the zirconium and theiron group metals readily unite to form homogeneous alloys of varyingcomposltion depending upon the relative quantities of the materialsemployed and the conditions of reduction. The alloys thus produced areof a type hitherto unknown among metallic zirconium combinations. Theyexhibit practically no tendency to oxidize and are highly resistant tomost chemical reagents. In appearance they are truly metallic, and theycan be produced in compact bodies which upon grinding and polishi areadapted to be worked up into shaped articles having utility in manyconnections.

A highly important application of these alloys is in the manufacture ofdrawn filaments, glowers or other luminescent bodies for electric lamps.In use, the filaments have the property of selective radiation, (that isemit more light than corresponds to the temperature) and may be used tomake lamps which require considerably less than the usual Wattage percandle power. They possess a remarkably high degree of luminescence atrelatively low filament tem peratures and are thus very eflicientsources of light. While other metals of the iron group than iron itself,such as nickel, cobalt, or manganese, or alloys or mixtures thereof, arecapable of se in the present invention, they are not in practice asdesirable as iron. For the present purposes, iron is by far the mostsatisfactory metal of the iron group. The relative proportions of ironand zirconium in alloys under the present' of zirconium in such binaryalloys are still more desirable for various reasons; and the alloys offrom approximately to 90 per cent. zirconium content with 40 to 10 percent. of iron are particularly advantageous.

The excellence of these zirconium alloys may be considerably enhancedand many desirable properties attained by the inclusion of a smallamount of titanium in the alloy, either by co-reduction of titanium withthe other constituents, or by separate addition of titanium toa'preformed alloy. The allowable amount of titanium so present is notrigidly restricted, but very small quantities prove eflicacious inpractice. As little as 0.10 per cent. serves the present purpose in someinstances, and it is seldom necessary in alloys for most purposes thatthe titanium content shall exceed 2 or 3 per cent. These small amountsof titanium give enhanced strength and toughness to the zirconiumalloys, and also increase their electrical properties. are also morepronounced. Furthermore in the manufacture of these alloys byco-reduction of the component metals, the presence of the titaniumcompounds in the mixture reduced has a useful efiect in preventing theundesirable retention of oxygen and oxygen compounds in the alloy orresultant melt. The presence of titanium also operates to excludenitrogen, carbon and other metalloids'from the alloy produced. Oxygenand other metalloids have an undesirable eifect on malleability,ductility and texture; Ternary alloys containing a certain amount oftitanium with preponderating proportions of zirconium and iron havecertain decided advantages over the simple b1- nary alloys for manypurposes.v Finally, the addition of small amounts of other metals suchas ,aluminum, tantalum, columbium, (niobium,) etc., give quaternary andstill more complex zirconium-iron alloys which for some purposes ofi'erparticular advantages and in them the relative proportions of zirconiumand iron may often, with advantage, vary more widely than in the simplebinary zirconium iron alloys. It is to be understood, however, that inall these alloys under the resent invention the combined zirconium-ironcontent preponderates over the other metals. Typical analyses ofquaternary alloys of the present invention comprising zirconium, iron,titanium and aluminum are as follows: zirconium 65.78%, 32.97%; iron26.39%, 90.97%, 49.21%; titanium 0.12%, 0.13%, 0.42%; aluminum 7.71%,-0.4:7%, 17.40%. 4

The described alloys are substantially iron-zirconium alloys, othermetals forming a minor fraction. And, for practical purposes, thesealloys may be looked upon as zirconium alloyed with iron or itsequivalent, an iron-rich ferrous alloy.

The ductility and malleability The process of making the describedalloys under the present invention is one of coreduction of compoundscontaining zirconium and iron in such a manner that the two metals arepresented to each other in a reaction being started with any firingmeans or materials such as magnesium, barium oxids, etc. In making analloy of iron and zirconium containing about 44.7 per cent. zirconiumthe following equation may serve to represent the. reaction of'reductionby aluminum:

( z) s'i' z s'i': 2) 3 The process of reduction may also be carried outby suitably heating the mixed oxids in a graphite crucible as by meansof the oxyacetylene flame, or electrically. Or, a mixture oftitaniferous oxid of iron, and the mineral zircon, or otherzirconiumcontaining materials, such as zirconia to gether with suitableamounts of titaniferous minerals such as rutile, ihnenite, sphene, ti.-

suitably shaping the alloys produced as' above described may be heatedto the necessary temperature, rolled, drawn, swaged or extruded throughdies to size, the alloy rod being conveniently heated by passage of acurrent therethrough during drawing. With many of the present alloys nospecial precautions need [be taken to avoid oxidation during working,but where necessary or desirable, working may be carried on in "vacuo orin an inert atmosphere.

In addition to their utility for incandescent lamp filaments and forglowers, alloys under the present invention may be usefully employed informing arcs. As stated, the present materials give out more light thanisequivalent to their temperature.

Being resistant to acids and corrosion, the

alloys may be used for various shaped articles for ornamental and otherpurposes,

such as spark points, etc. Another field of utility for these alloys isin the manufacture of transformer elements.

Halogen compounds, such as fluorids, chlorids, etc., of the variousmetals may be used in making the alloys by co-reduction; but their useoffers no advantage over that of the employment of the oxidizedcompounds of the metals as described.

What I claim is 1. As a new article, an alloy comprising not less thanabout 40 per cent. and not more than about 90 per cent. zirconiumtogether with an iron group metal.

52. As a new article, an alloy comprising not less than about 40 percent.- and not more than about 90 per cent. zirconium together withiron.

3. As a new article, an alloy comprising approximately between 60and 90per cent. zirconium together with an iron group metal.

4. As a new article, an alloy comprising approximately between 60 and 90per cent. zirconium together with iron.

5. An alloy comprising between 60 and 90 per cent. zirconium, theresidue of said alloy being mainly iron, and said alloy beingsubstantially free of oxygen, oxids and metalloids and being malleableand ductile.

6. The process of making an alloy comprising iron and zirconium whichcomprises admixing materials containing compounds of iron and ofzirconium and co-reducing the metals from the mixture as an alloy.

7. The process of making an alloy comprising'iron and zirconium whichcomprises admixing materials containing compounds of iron, of zirconiumand of titanium and co-reducing the metals from the mixture as an alloy.

8. The process of making an alloy comprising iron and zirconium whichcomprises admixing materials containing compounds of iron and ofzirconium fwith metallic aluminum and igniting the mixture.

In testimony whereof, I aflix my signature in the presence of twosubscribing witnesses.

JOHN LOUIS BROWN. Witnesses:

HOWARD S. SHELDS, E. R. COOPER.

